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Concurrent supercritical fluid chromatographic analysis of terpene lactones and ginkgolic acids in Ginkgo biloba extracts and dietary supplements

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Abstract

Supercritical fluid chromatography was used to resolve and determine ginkgolic acids (GAs) and terpene lactones concurrently in ginkgo plant materials and commercial dietary supplements. Analysis of GAs (C13:0, C15:0, C15:1, and C17:1) was carried out by ESI (−) mass detection. The ESI (−) spectra of GAs simply displayed only the [M-H]− pseudo-molecular ions, and selected ion monitoring (SIM) for those ions was used for the quantification. Analysis of terpene lactones (ginkgolides A, B, C, J and bilobalide) was complicated by in-source collision-induced dissociation (IS-CID) in the ESI source. Thus, MS analysis could be influenced by the fragmentation pattern produced by the IS-CID. However, it was established that the fragmentation pattern, measured by ion survival yield (ISY), was independent of analyte concentration or matrix at a fixed cone voltage in the ESI source. Therefore, MS with SIM mode was applicable for the analysis of these analytes. The reported method provided consistent and sensitive analysis for the analytes of interest. The LOQs and LODs were determined to be below 100 and 40 ng/mL for GAs and 1 μg/mL and 400 ng/mL for terpene lactones, respectively. Intra- and inter-day precisions were found to be satisfactory with RSDs being below 5.2 %. Analyte recoveries ranged from 87 to 109 %. The developed method was successfully applied to the analysis of 11 ginkgo plant samples and 8 dietary supplements with an analysis time of less than 12 min.

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Acknowledgments

This research is supported in part by “Science Based Authentication of Dietary Supplements” funded by the Food and Drug Administration grant number 1U01FD004246-05 and The United States Department of Agriculture, Agricultural Research Service, Specific Cooperative Agreement No. 58-6408-1-603-07.

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Authors and Affiliations

  1. National Center for Natural Products Research, School of Pharmacy, University of Mississippi, University, MS, 38677, USA

    Mei Wang, Emily J. Carrell, Amar G. Chittiboyina, Bharathi Avula, Yan-Hong Wang, Jianping Zhao, Jon F. Parcher & Ikhlas A. Khan

  2. Division of Pharmacognosy, Department of BioMolecular Science, School of Pharmacy, University of Mississippi, University, MS, 38677, USA

    Ikhlas A. Khan

  3. Department of Pharmacognosy, College of Pharmacy, King Saud University, Riyadh, 11451, Saudi Arabia

    Ikhlas A. Khan

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  1. Mei Wang
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Correspondence to Ikhlas A. Khan.

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Wang, M., Carrell, E.J., Chittiboyina, A.G. et al. Concurrent supercritical fluid chromatographic analysis of terpene lactones and ginkgolic acids in Ginkgo biloba extracts and dietary supplements. Anal Bioanal Chem 408, 4649–4660 (2016). https://doi.org/10.1007/s00216-016-9544-6

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